An isomeric mixture ofp-butyl-p'-methoxy-azoxybenzenes (IV) and the low melting eutectic mixture ofp-butyl-p'-methoxy-azoxybenzenes withp-ethyl-p'-methoxy-azoxybenzenes (V) have been analyzed with differential scanning calorimetry (DSC). By quenching, it was possible to establish the glassy mesophase of both materials. Their glass transition temperatures are 207.6 K and 208.1 K, respectively, with an increase in heat capacity atTgof 129 JK−1mol−1and 102 JK−1mol−1. As found previously with polymeric mesophases, the hysteresis is strongly reduced, while the ΔCpseems little affected by going from an amorphous glass to a mesophase glass. The melting, cold crystallization, and mesophase-isotropic melt transitions were also studied.